Warning
This document is not an ISO International Standard. It is distributed for review and comment. It is subject to change without notice and may not be referred to as an International Standard.
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Contents

1 Scope ..................................................................................................................................................1
　1.1 General ...............................................................................................................................................1
　1.2 Substance determined ........................................................................................................................1
　1.3 Type of sample ...................................................................................................................................1
　1.4 Range ..................................................................................................................................................2
　1.5 Limit of detection ...............................................................................................................................2
2 Normative references .........................................................................................................................2
3 Principle ..............................................................................................................................................2
4 Terms and definitions .........................................................................................................................2
5 Symbols and abbreviated terms ........................................................................................................6
6 Sample collection ...............................................................................................................................6
　6.1 Requirements .....................................................................................................................................6
　　6.1.1 Sampling apparatus ............................................................................................................................6
　　6.1.2 HEPA vacuum cleaner ........................................................................................................................7
　　6.1.3 Materials and supplies for sampling .................................................................................................7
　6.2 Procedure ...........................................................................................................................................8
　　6.2.1 Safety precautions ..............................................................................................................................8
　　6.2.2 Sample size requirements ..................................................................................................................8
7 Sample preparation ........................................................................................................................... 11
　7.1 General ............................................................................................................................................. 11
　7.2 Removal of organic materials by ashing ......................................................................................... 11
　7.3 Removal of soluble constituents by acid treatment ....................................................................... 11
　7.4 Sedimentation and flotation ............................................................................................................. 11
　7.5 Combination of gravimetric reduction procedures ........................................................................ 11
8 Analysis by PLM ............................................................................................................................... 11
　8.1 Requirements ................................................................................................................................... 11
　　8.1.1 Stereo-binocular microscope ........................................................................................................... 11
　　8.1.2 Polarized light microscope ............................................................................................................... 11
　　8.1.3 Dust extract hood .............................................................................................................................. 12
　　8.1.4 Sample preparation ........................................................................................................................... 12
　8.2 Qualitative analysis by PLM ............................................................................................................. 15
　　8.2.1 Calibration ........................................................................................................................................ 15
　　8.2.2 Sample preparation ........................................................................................................................... 16
　　8.2.3 Sample analysis ............................................................................................................................... 16
　　8.2.4 Interferences .................................................................................................................................... 23
9 Analysis by SEM ............................................................................................................................... 25
　9.1 Requirements ................................................................................................................................... 25
　　9.1.1 Scanning electron microscope ........................................................................................................ 25
　　9.1.2 Energy dispersive x-ray system ...................................................................................................... 25
　　9.1.3 Vacuum coating unit ......................................................................................................................... 25
　9.2 Calibration ........................................................................................................................................ 25
　9.3 Sample preparation ........................................................................................................................... 26
　9.4 Qualitative analysis by SEM ............................................................................................................. 26
　　9.4.1 Sample analysis ............................................................................................................................... 26
10 Analysis by TEM ............................................................................................................................... 28
　10.1 Requirements ................................................................................................................................... 28
　　10.1.1 Transmission electron microscope ................................................................................................. 28
　　10.1.2 Energy dispersive X-ray analyzer .................................................................................................... 28
　　10.1.3 Vacuum coating unit ......................................................................................................................... 28
　　10.1.4 Calibration grids for EDXA ............................................................................................................... 28
　　10.1.5 Disposable tip micropipettes ........................................................................................................... 28
　10.2 Calibration ........................................................................................................................................ 28
　10.3 Sample preparation.......................................................................................................................... 29
　10.4 Qualitative analysis by TEM ............................................................................................................. 29
　　10.4.1 Chrysotile ......................................................................................................................................... 29
　　10.4.2 Amosite ............................................................................................................................................. 29
　　10.4.3 Crocidolite ........................................................................................................................................ 29
　　10.4.4 Tremolite ........................................................................................................................................... 29
　　10.4.5 Actinolite .......................................................................................................................................... 30
　　10.4.6 Anthophyllite .................................................................................................................................... 30
　　10.4.7 Sodic-calcic amphibole asbestos (richterite/winchite) .................................................................. 30
11 Test report ........................................................................................................................................ 30

Annex A (normative) Types of commercial asbestos-containing material .............................................. 33
Annex B (normative) Interference colour chart .......................................................................................... 40
Annex C (normative) Dispersion staining charts ....................................................................................... 41
Annex D (normative) Identification of asbestos by PLM and dispersion staining in commercial asbestos-containing materials ... 44
Annex E (normative) Identification of asbestos by SEM in commercial asbestos-containing materials ... 53
Annex F (normative) Identification of asbestos by TEM in commercial asbestos-containing materials ... 59
Annex G (informative) Example of sampling record .................................................................................. 65
Annex H (informative) Example of analysis report .................................................................................... 66

Introduction

In the past, asbestos was used in a wide range of products. Materials containing high proportions of asbestos were used in buildings and in industry for fireproofing, thermal insulation and acoustic insulation. Asbestos was also used to reinforce materials, to improve fracture and bending characteristics. A large proportion of the asbestos produced was used in asbestos-cement products. These include flat sheets, tiles and corrugated sheets for roofing, pipes and open troughs for collection of rainwater, and pressure pipes for supply of potable water. Asbestos was also incorporated into products such as decorative coatings and plasters, glues, sealants and resins, floor tiles, gaskets and road paving. In some products asbestos was incorporated to modify rheological properties, for example in the manufacture of ceiling tile panels and oil drilling muds.

Three varieties of asbestos found extensive commercial application. Chrysotile accounted for approximately 95% of consumption, and therefore this is the variety that is encountered most frequently during analysis of samples. Amosite and crocidolite accounted for almost all of the balance, with a very small contribution from anthophyllite. Amosite was generally used as fireproofing or in thermal insulation products. Crocidolite was
also used as fireproofing and thermal insulation products, but because it is highly resistant to acids, it also found application as a reinforcing fibre in acid containers such as those used for lead-acid batteries, and in some gaskets. Materials containing commercial anthophyllite are relatively rare, but it also has been used as a filler and reinforcing fibre in composite materials, and as a filtration medium. Tremolite asbestos and actinolite asbestos were not extensively used commercially, but they sometimes occur as contamination of other commercial minerals. Richterite asbestos and winchite asbestos occur at concentrations between 0.1% and 6% in vermiculite formerly mined at Libby, Montana, U.S.A. Vermiculite from this source was widely distributed and is often found as loose fill insulation and as a constituent in a range of construction materials and fireproofing.

While the asbestos concentration in some products can be very high and in some cases approach 100%, in other products the concentrations of asbestos used were significantly lower and often between 1% and 15%. In some ceiling tile panels, the concentration of asbestos used was close to 1%. There are only a few known materials in which the asbestos concentration used was less than 1%. Some adhesives, sealing compounds and fillers were manufactured in which asbestos concentrations were lower than 1%. There are no known materials in which asbestos was intentionally added at concentrations lower than 0,1%.

In Part 1 of this standard, procedures for collection of samples and procedures for qualitative analysis of commercial bulk materials for the presence of asbestos are specified. A visual estimate of the asbestos concentration may also be made, but it is recognized that the accuracy and reproducibility of such estimates is very limited. For practical purposes, since no known commercial materials exist in which commercial
asbestos was intentionally added at concentrations lower than 0,1%, Part 1 of this standard specifies that samples be classified as asbestos-containing (i.e. containing more than 0,1% asbestos) if either chrysotile, amosite, crocidolite, or anthophyllite, or any of these varieties in combination, is detected in the analysis. Because of the wide range of matrix materials into which asbestos was incorporated, polarized light
microscopy cannot provide reliable analyses of all types of asbestos-containing materials in untreated samples. The applicability of polarized light microscopy can be extended by the use of simple treatments such as ashing and treatment with acid. However, there are some classes of commercial asbestos-containing material that cannot be reliably analyzed by polarized light microscopy. The occurrence of tremolite, actinolite
or richterite/winchite in a material is usually as a consequence of natural contamination of the constituents, and the detection of these minerals does not necessarily indicate that the concentration is more than 0,1% asbestos. Accordingly, classification of these minerals as asbestos-containing by the 0,1%criterion can only be achieved by quantitative analysis. Since these minerals were not specifically mined and utilized for their fibrous properties, they may occur in materials as either non-asbestiform or asbestiform analogues, or mixtures of both.

Other parts of this standard specify procedures for quantification of asbestos concentrations below approximately 5%, and quantitative determination of asbestos in vermiculite, other industrial minerals and commercial products that incorporate these minerals.

In Part 1 of this standard, the primary method for identification of asbestos is polarized light microscopy. Optionally, either scanning electron microscopy or transmission electron microscopy may be used as an alternative or confirmatory method to identify asbestos. It is recognized that asbestos-containing materials are defined in some jurisdictions as materials containing more than 0.5% or more than 1% by weight of asbestos. Some commercially manufactured materials are known in which asbestos was intentionally added at concentrations that may have been either lower than or higher than these defined control limits. For these specific types of asbestos-containing material, it may be necessary to proceed to other parts of this standard in order to quantify the asbestos for the purpose of defining the regulatory status of the material.

This method is based on MDHS 77 [1], VDI 3866 Part 1 [2], VDI 3866 Part 4 [3], VDI 3866 Part 5 [4], AS 4964-2004 [5] and EPA/600/R-93/116 [6].

Table 3. Optical properties of NIST SRM 1866 and SRM 1867 reference asbestos samples NOTE * For crocidolite, the NIST certificate of analysis states: "Because strong absorption in the visible light range results in anomalous dispersion characteristics that would not be useful to the analyst, no certified values of refractive index are reported for riebeckite." Table 4. Optical properties of IOM/HSE reference asbestos samples Figure C.1 . Dispersion staining chart for chrysotile in 1.550 RI liquid. Figure C.2 . Dispersion staining chart for amosite in 1.680 RI liquid. Figure C.3 . Dispersion staining chart for crocidolite in 1.700 RI liquid Figure C.4 . Dispersion staining chart for tremolite in 1.605 RI liquid. Figure C.5 . Dispersion staining chart for actinolite in 1.630 RI liquid. Figure C.6 . Dispersion staining chart for anthophyllite in 1.605 RI liquid. Figure C.7 . Dispersion staining chart for richterite/winchite asbestos in 1.630 RI liquid. ISO（2007）による『Bulk materials−−Part 1: Sampling and qualitative determination of asbestos in commercial bulk materials』から